Method of making stannic chlorid.



PATENTED MAR. 17, 1908.

E. A. SPERRY.

METHOD OF MAKING STANNIG CHLORID.

APPLICATION FILED NOV. 23. 1905.

2 SHEETS-SHEET 1.

PATENTED MAR. 17, 1908.

E. A. SPERRY. METHOD OF MAKING STANNIO GHLORID.

APPLICATION FILED 110123. 1905.

2 SHEETS-SHEET 2.

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UNITED STA1 E S PATENT OFFICE.

ELMER A. SPERRY, OF BROOKLYN, NEW YORK, ASSIGNOR T CHEMICAL REDUCTIONCOM- PANY, OF NEW YORK, N. Y., A CORPORATION 01 NEW YORK.

METHOD OF MAKING STANNIC CHLORID.

Specification of Letters Patent.

Patented March 17, 1908.

Application filed November 23, 1905. Serial No. 288,780.

To all whom it may concern:

Be it known that I, ELMER A. SPERRY, a citizen of the United States,residing at Brooklyn, in the county of Kings and State 5 of New York,have invented certain new and useful Im movements in Methods of MakingStannic hlorid, of which the following is a specification.

This invention is a method of treating metallic tin or bodies containingthe same to produce compounds of tin and particularly the anhydrous andhydrated stannic chlorids. According to my invention a materialconsisting wholly or in part of metallic tin, here inaiter referred toas a tin-bearing material,

is subjected to the action of chlorin in any of its reacting conditions,that is to say as gaseous chlorin, mixed or not with air, water or watervapor or other ases dissolved chlorin, as, for instance, a solution ofchlorin in anhydrous or hydrated stannic chlorid; or liquid chlorin. Themethod of treatment is the same in essential particulars in all cases,in that the chlorin is brought into reacting relation with metallic tinunder conditions which admit of temperature control. 'lhe reaction iscarried out in inclosed vessels which may be placed in series or inmultiple relation.

As a specilicexample of my method 1 will describe the production ofchlorids of tin by reacting on a tin-bearing material with chlorindissolved in chlorid of tin. it being understood that the invention isnot limited to this particular procedure.

For a full understanding ol" my invention reference is made to theaccompanying drawings wherein Figure l shows in side elevation anarrangement ol' apparatus for carrying out my invention. parts beingbroken away: and Fig. i is a diagr; in illust ralivc ol' my method.

lieicrring to Fig. l: l, 2, Ii are reaction vessels which are shown asconneclcd in se rics but which may b used singly. 'lhese vessels may beol iron. lead or ollur suitable material. and are jacketed as indicatedat 4, means comprising a pipe-system and a iump (i being provided forcirculating a 50 mating or cooling medium, as water, through the jacketsol' the several yesscls, thereby cll'ccting a iransl'cr of heat betweenthe several reacting bodies; this is of advantage since the heat fromthe bodies at higher tomperature is transferred in part to those oflower temperature, thereby equalizing the temperatures throu hout thesystem. This arrangement is employed when a number of vessels are usedwhether the vessels are connected in series or in multiple.

7 is a device for heating or coolin the circulating medium as may berequired, the temperature of the circulating medium being so regulatedas to withdraw heat during the reaction period and to supply heat duringthe subsequent distillation of stannic chlorid.

8 is an inlet for chlorin, with which air and other gasesand water or\\"atervapor are commonly associated. Tin in bar, powder or other formis introduced from time to time through suitable covered apertures 9,and during the major portion ol the reaction period a considerableexcess of the metal should be present. The products of the reactionremaining from the distillation are withdrawn as required through valvedpipes 10 which may conveniently communicate with the common dischargepipe 1 l.'

When moisture is present in the chlorin or is admitted therewith theproduct will consist ol' anlrvdrous and hydrated chlorids of tin, theproportion ol these chlorids being governed by the proportion olmoisture in the chlorin. l have found that a certain proportion ol'moisture is :ulvantageous in practice, since the solution ol tin isaccelerated by its presence or by the presence oi the hydrated chloridresulting from its combination. The temperature of the reacting mass ispreferably maintained at such degree as to avoid substantial separationof the hydrated stannic chlorid, this temperature varying somewhat inaccordance with the character ol the material under treatment and theproportion ol hydrated chlorid present, and being controlled by thetemper-at ure. ol' the circulating liquid. Under these temperatureconditions the several chlorids are liquid and are readily witlulrawnfrom the reaction vessels carrying with them any solid residues.Preferably these mixed liquid chlorids are 'lillered or strained l'romany foreign matter or undissolvcd residue. while hot and are thenpermitted to cool, whereupon the hydrated chlorid crystallizes out as amarketable prmluct, rccrystallization or other method ol" purificationbeing resorted to if necessary. The undissolved residue may or may befurther purified by distillation.

When an excess of chlorin is used, or when the chlorin is diluted oradmixed 'With air, carbon dioxid, moisture, etc.,. as is commonly thecase, the residual gases passing from the reaction'vessel are charged orsaturated with chlorid of tin. These gases are preferably cooled, as incondensers 12, 12, conveniently arranged in communicating pairs asindicated, whereby a separation of both anhydrous and hydrated chloridoccurs. The anhydrous chlorid is collected as in vessels 13, and anychlorin separated as hereinbefore described; the hydrated chlorid isremoved from the condensers through outlets 14 in the form of crystalsand is added to thatrecovered from the reaction vessels.

The separation of chlorid of tin from the uncondensed gases in thecondensers is ordinarily incomplete, and the final portions arepreferably removed by leading the gases into contact with water or othersolvent in a tower or scrubber 15. I have found it preferable inpractice to subject these gases to the action of the solvent atsuccessively higher and' lower temperatures, as,.for instance, byadmitting hot water through the lower inlet or spray 16, and cold waterthrough the upper inlet 17, whereby all traces of tin compounds areseparated; obviously communicating scrubbers for hot and cold Water orsolvent, respectively, may be used, or equivalent means may be used toeflect the same result. The product from the tower 1 5, collectedas at18, is a stannic chlorid solution the concentration of which Willobviously depend upon the proportion of the water used to the stannicchlorid in the vapors; No difficulty is experienced in preparing thesolution of 5060 1%., if desired, such solution being a marketableproduct.

The exhaust fan 19 for the residual gases serves to maintain adiminished pressure in the tower 15 as compared with the pressure in"the reaction vessels, and thereby to insure a movement of the gasesthrough the system.

Fig. 2 expresses in diagrammatic form the several reactions andseparations which 00- curand the disposition of the products as hereinset forth.

The expression liquid hydrated stannic chlorid occurring in the claimsrefers to a hydrated stannic chlorid liquefied by heat or existing aboveits temperature of solidification or separation, and does not Include anaqueous solution of stannic chlorid.

- a I claim:

1. The method of producing stannic chlorid Which consists in bringingchlorin into contact with a body of tin-bearing material 3. The methodof producing stannic chlo- I rid which consists in reacting on atin-bearing material with chlorin containing mois ture as a diluentinthe resence of anhydrous stannic chlorid and'cooling-the reacting mass.I 4. The method of producing stannic chlorid whicheonsists'in reactingon a tin-bear ing material with chlorin containing moisture' and air asdiluents in the presence of anhydrous stannic chlorid and cooling thereacting mass.

5; The method of producing stannic chloridwhich consists in reacting ona tin-bear-' ing material with free chlorin in presence of liquidhydrated stannic chlorid.

6. The method of producing stannic chlorid which consists in reacting ona tin-bearing material with tree chlorin in presence of liquid hydratedstannic chlorid and anhy-- drous stannic chlorid.

7. The method of producing stannic chlorid which consists in reacting ona tin-bearing material with chlorin in the presence of water in quantityinsufficient to produce solu tion, forming thereby anhydrous andhydrated stannic chlorids, vaporizing such chlorids and condensing them.

8. The method of producing stannic chlorid which consists in reacting ona tin-bearing material with chlorin in the presence of water in quantityinsuflicient to produce solution, forming thereby anhydrous and hydratedstannic chlorids, vaporizing such chlorids and condensing them, andbringing the residual ases into contact with a solvent for stannicdhlorid.

9. The method of producing stannic chlorid which consists in reacting ona tin-bearing material with chlorin in the presence of water in quantityinsullicient to produce solution, forming thereby anhydrous and hydratedchlorids of tin, and controlling the temperature of the reaction.

10. The method of producing stannic water in quantity insuiiicient toproduce so-' lution, producing thereby anhydrous and hydrated, stannicchlorids, separating said chlorids from each other, and separating thechlorin from the anhydrous chlorid.

13. The method of producing stannic chlorid which'consists it. reactingon a tinbearing material with chlorin in presence of water in quantityinsullicient to produce solution, maintaining the temperature duringreaction above the melting point of the hydrated chlorid, then coolingthe mixture and se )arating the anhydrous ar. d hydrated chlorir s fromeach other.

14. The method of producing stannic chlorid which consists in bringingchlorin into contact with a tin-bearing material and producing anhydrousstannic chlorid, maintaining the stannic chlorid substantially,saturated with free chlorin, condensing and collet-ting stannicchlorid, and brfnging the re- I sidual gases into contact with, asolvent tor stannicchlorid.

15. The method of producing stannic chlorid which consists in reactingon a tinbearing material with diluted chlorin, producing anhydrousstannic chlorid, condensing and collecting the same and bringing theresidual gases into contact with a solvent therefor at successivelyhigher and-lower temperatures.

16. The method of producing stannic chlorid which consists in reactingon a tin bearing material with chlorin condensing anhydrous stannicchlorid from the vapors and bringing the residual va )ors into contactwith a solvent therefor un er pressure less than that ol' theatmosphere.

17. The method of making stannic chlorid which consists in reacting withchlorin on a tin-bearing i'naterial containing foreign mat ter,volatilizing part of said chlorid, and separating any remaining chloridfrom the residue by the action ol a solvent.

18. The method 1 of producing stannic chlorid which consists in reactingwith chlorin on separate bodies ol" tin-bearing material and ell'ectinga transfer of heat. between said bddies by means of a medium out ofcontact therewith.

19. The method (it making stannic chlorid which consists in reactingwith chlorin on a tin-bearing material in presenceof a body of liquidanhydrous s1; annic chlorid cooling said body during the reactionperiod, vaporizing stannic chlorid from said body, and eondens ing same.

20. The method ol" mahing stannic chlorid which consists in reactingwith chlorin on a tin-bearing material in presence of a body ol" liquidanhydrous stannic chlorid cooling said body during the reaction period,vaporizing stannie chlorid from said body while in the reaction vessel,and condensing same.

21. The method of making stannic chlorid which consists in reacting on atin-bearing material with chlorin in presence o'l anhydrous stannicchlorid at a tr'nnperature below the vaporizing point cl stannicchlorid, main taining the reaction by supplying chlorin to the reactingmass, and separating the stannic chlorid from the nndissolved residue bytractional distillation. V

In testimony whereof, I allix my signature in presence of two witnesses.

ELMER A. SPlQltltY.

\Vitnesses:

